Guys I screwed up...

[kurtak]

Most of the salts will be water-soluble and dissolve in water.

:shock: --- that does not make sense - he has already "added" baking soda to his solution - enough baking soda that he precipitated carbonites/carbonates - which means he has raised the Ph (how much we don't know)

Simply adding (diluting) with water is not going to dissolve those salts - if anything it "may" allow more salts to fall out

until we know the PH of his solution after he added the baking soda we can't "fully" advise him on how to proceed

Depending on the Ph - I "might" just filter out the solids & then hit the filtered solids with HCl

From what I see - he has gold in those solids (how much we do not know) as the result of "first" adding SMB - then adding baking soda

When he added the baking soda - he may have (or not) killed most &/or all of the nitric - so depending on that - when he hits the solids with HCl - he may dissolve just the salts leaving the gold - or dissolve the salts & "some" gold (but leave some) - or dissolve both the salts & all the gold

Filtering out the solids "should" allow him to use less acid - why? --- because he only needs enough acid to dissolve the solids & NOT have to adjust the Ph of the solution "before" the HCl "starts" also dissolving the solids

The (filtered) solution --- need to know two things - what is the Ph - & what is the stannous test

From what I see - stannous shows a "trace" of gold - because it's a trace - again - I would want to know the Ph before I decided on how to recover that "trace" --- in other words - depending on Ph - do I need to lower the Ph to recover that trace - or can I recover it as is (&/or a couple other options I see with that solution)

In other words - I don't quite get why we are going around & around here without know what the Ph is as a result of his adding baking soda ?

Goldman94 - bottom line - if you are going to get into refining - besides having stannous in your tool box - you need to have a way to test Ph --- you don't need a Ph test "kit" &/or a Ph meter - but you at "least" need Ph test paper - you want the Ph test paper to be good for testing in the range from Ph 1 - Ph 13

if nothing else you need to be able to test Ph when you go to treat (adjust) your waste solution for "proper" disposal - can't just dump them down the drain - so get some Ph paper

Kurt

 

[kurtak]

STOP. You're digging yourself into a bigger and bigger hole. At this point I think you should filter your solutions and put the liquids and solids to the side. If you go this route I can help you. If not your just going to keep spinning your wheels.

:lol: :lol: :lol:

The SHORT version posted before I posted :mrgreen:

Kurt

 

[Goldman94]

Okay, so I just tested the solution with stannous and the results came back negative for gold. With all the sediment I see, it seems like a decent amount has precipitated out as gold flakes and a little brown powder (from what I see in the salts)

With how much baking soda I used, I believe I killed off all the nitric, since i only used about 10ml, but I cant be positive of that.

As for the ph test, I'll go today and get one. What do I need to know about that?

I think I will just filter off the clear yellow solution and keep the solids to the side. So keeping that to the side, should I add HCL until it's all gone?

 

[Shark]

By adding the sodium bicarbonate, that would kill not just the nitric but the hydrochloric as well.


As Kurt mentioned, you need to be able to test from Ph1 to Ph13. Swimming pool test paper won't go to the extreme high or low side, so they won't work for a full range of testing. I have a couple of digital PH meters that I got at a large nursery for testing soil acidity. They might not last long, but they can be bought for around $10. The one I like best of the two is made by Jellas, and I have been using it for over a year now. If you have a brewing shop near by they will sometimes carry a full line of Ph test papers and sometimes digital meters as well.

 

[Goldman94]

By adding the sodium bicarbonate, that would kill not just the nitric but the hydrochloric as well.


As Kurt mentioned, you need to be able to test from Ph1 to Ph13. Swimming pool test paper won't go to the extreme high or low side, so they won't work for a full range of testing. I have a couple of digital PH meters that I got at a large nursery for testing soil acidity. They might not last long, but they can be bought for around $10. The one I like best of the two is made by Jellas, and I have been using it for over a year now. If you have a brewing shop near by they will sometimes carry a full line of Ph test papers and sometimes digital meters as well.

I'm guessing I need a ph around 1? But if I just keep adding HCL and try to get rid of the baking soda by adding more and more HCL wont that work too?

 

[FrugalRefiner]

You keep talking about treating all your solution or all your solids, but you have no idea what you have. When dealing with an unknow, the best tactic is to do some testing on SMALL amounts of each. When I say small, I mean test tube tests. So you would take a SMALL sample of your solids, put them in a test tube, then put in small amounts of HCL etc. to see what happens. When you find a method that works, then you can apply it to the rest of the batch.

You can buy wide range pH test papers on eBay for around a dollar.

Personally, I would advise you to set your mess aside and study. Reread this thread. Obviously there is a lot that has been said that you do not understand. Study till all the advice makes sense. Then when your pH papers arrive, you can pull your mess back out and proceed with some hope of getting your gold back out.

Dave

 

[Goldman94]

You keep talking about treating all your solution or all your solids, but you have no idea what you have. When dealing with an unknow, the best tactic is to do some testing on SMALL amounts of each. When I say small, I mean test tube tests. So you would take a SMALL sample of your solids, put them in a test tube, then put in small amounts of HCL etc. to see what happens. When you find a method that works, then you can apply it to the rest of the batch.

You can buy wide range pH test papers on eBay for around a dollar.

Personally, I would advise you to set your mess aside and study. Reread this thread. Obviously there is a lot that has been said that you do not understand. Study till all the advice makes sense. Then when your pH papers arrive, you can pull your mess back out and proceed with some hope of getting your gold back out.

Dave

It's not that I haven't studied any of this. I just made 1 costly mistake. If I never would have added the baking soda, I never would have been in this predicament.

 

[Shark]

By adding the sodium bicarbonate, that would kill not just the nitric but the hydrochloric as well.


As Kurt mentioned, you need to be able to test from Ph1 to Ph13. Swimming pool test paper won't go to the extreme high or low side, so they won't work for a full range of testing. I have a couple of digital PH meters that I got at a large nursery for testing soil acidity. They might not last long, but they can be bought for around $10. The one I like best of the two is made by Jellas, and I have been using it for over a year now. If you have a brewing shop near by they will sometimes carry a full line of Ph test papers and sometimes digital meters as well.

I'm guessing I need a ph around 1? But if I just keep adding HCL and try to get rid of the baking soda by adding more and more HCL wont that work too?

Don't guess.

You have butcher, kurtack, goldenchild and Frugalrefiner, trying to guide you. Short of getting a full education in chemistry it don't get much better than than that.

 

[Goldman94]

I know, and they've been way more than helpful and I'm so grateful for all the knowledge that they've shared with me.

I just want to get this mess figured out and recover this stupid gold

 

[jimdoc]

I just want to get this mess figured out and recover this stupid gold

Gold is never stupid. Now tin, tin can get stupid.

 

[Goldman94]

I just want to get this mess figured out and recover this stupid gold

Gold is never stupid. Now tin, tin can get stupid.

Lol...I'm just scared to see what my recovery will be when it comes to it. Im expecting close to 10g but I have a funny feeling it won't be close

 

[butcher]

Most of the salts will be water-soluble and dissolve in water.


:shock: --- that does not make sense - he has already "added" baking soda to his solution - enough baking soda that he precipitated carbonites/carbonates - which means he has raised the Ph (how much we don't know)

Simply adding (diluting) with water is not going to dissolve those salts - if anything it "may" allow more salts to fall out

Kurt,
Maybe I used the wrong word, (most), well maybe not most of those salts will be water-soluble, but well, a heck of a lot of the salts will be water-soluble after evaporating the solution down to salts, such as the NaCl, NaNO3 created from the HCl and nitric in solution reacting with the sodium bicarbonate...

The HCl acid would have formed soluble sodium chloride salt.
Any nitric would have formed sodium nitrate salts NaNO3.

Nitrate salts are generally water-soluble.
Chloride salts are generally water-soluble, except for silver, lead, and mercury chlorides.
Sulfate salts are generally water-soluble, except for lead and silver.
Carbonates are frequently insoluble in water.
Many of the base metal carbonate salts and gold will not be soluble in water...

Although many of the salts are water-soluble using HCl will dissolve more of the salts, than water alone will.
The HCl is mostly water anyway, and it also produces water in the chemical reactions with many of the salts, which will assist in dissolving the water-soluble salts, HCl will also help to convert much of the copper carbonates or other base metals into water-soluble chlorides...

You keep talking about treating all your solutions or all your solids, but you have no idea what you have. When dealing with an unknown, the best tactic is to do some testing on SMALL amounts of each. When I say small, I mean test tube tests. So you would take a SMALL sample of your solids, put them in a test tube, then put in small amounts of HCL, etc. to see what happens. When you find a method that works, then you can apply it to the rest of the batch.

You can buy wide-range pH test papers on eBay for around a dollar.

Personally, I would advise you to set your mess aside and study. Reread this thread. Obviously there is a lot that has been said that you do not understand. Study till all the advice makes sense. Then when your pH papers arrive, you can pull your mess back out and proceed with some hope of getting your gold back out.

Dave

 

[Goldman94]

Little update...

Here's one of the beakers, this one had the most salts in it so I decided to put some water in there and it really dissolved a lot of the solids. I'm really curious as to what this powder is now. Theres a fine layer of metallic gold on the bottom that is covered in a brownish powder but it doesnt really look like gold powder. It does and doesn't, if that makes any sense. I'm really tempted to try and melt some of it down and actually find out whether or not it is gold powder. It has a very fine consistency to it but it settles very quick to the bottom.

 

[butcher]

Don't melt any down at this point you could put your gold up in smoke and make it harder to get back.

It is doubtful the gold dissolved when you added water, but I would do a stannous test of the solution to confirm (I would also check pH and make sure it was at least somewhat acidic before doing a stannous test).

After decanting adding HCl, will begin to dissolve more of the salts, but also could put some gold in solution, that is if some of the salts are nitrates which may form a poor-mans aqua regia as you add HCl (so the stannous tests will be much more important to determine if the gold is being dissolved back with the salts and other base metals).

Basically, if water dissolves most of the salts, and you only have a little salt left with the gold just wash the gold (Search for the thread "getting my gold pure and shinning" use Harold as the author in your search).

After most of the salts were gone, and washing the gold,I would dissolve it back into solution for a proper (or second refining), studying the process well before beginning, and using the sulfamic Lou told you to invest in, if necessary...

Let solutions with gold powders in them settle overnight, and the solution to clear as much as possible before decanting, some salts take time to settle like fluffy silver chlorides and letting the dilute solution set in the cold of the night, will usually leave you with a little more of the salt in the morning

 

[Goldman94]

Don't melt any down at this point you could put your gold up in smoke and make it harder to get back.

It is doubtful the gold dissolved when you added water, but I would do a stannous test of the solution to confirm (I would also check pH and make sure it was at least somewhat acidic before doing a stannous test).

After decanting adding HCl, will begin to dissolve more of the salts, but also could put some gold in solution, that is if some of the salts are nitrates which may form a poor-mans aqua regia as you add HCl (so the stannous tests will be much more important to determine if the gold is being dissolved back with the salts and other base metals).
Basically, if water dissolves most of the salts, and you only have a little salt left with the gold just wash the gold (Search for the thread "getting my gold pure and shinning" use Harold as the author in your search).

After most of the salts were gone, and washing the gold,I would dissolve it back into solution for a proper (or second refining), studying the process well before beginning, and using the sulfamic Lou told you to invest in, if necessary...

I've been boiling what I think is my good batch, the one that was yellow and had the majority of gold in it, with just distilled water, since HCL wasn't doing anything at all. The moment I put water in it, half of the salt dissapeared and now I'm on my 2nd boiling and it's starting to form Crystals at the top. I just decanted that solution into another beaker and put more water in to try and rid the sludge of any salts.

Obviously I'm going to wait awhile until I think most of it is gone and then do a batch of AR and throw it in there and hope I strike gold.

As for my brown solution, I think I'm going to have to continue boiling it down and adding water to it to try and achieve the same thing as this one.

I'm saving all of my decanting solutions just incase anything was left behind, because I'm sure there was

 

[butcher]

I do not understand why your working with two batches?
It is hard for me to follow all of what is going on, I thought you were working with one mess, not two different batches.

Well as long as you understand what your doing.

After collecting all of your washes and solutions (even if they test negative for gold) you will not lose your gold if you follow the instructions to treat your waste for disposal properly. found in the safety section...

Any gold will cement out with copper. You will recover it in this step.
Copper and many of the other toxic base metals are cemented out with an iron.
Many more of the toxic metals are removed by raising the pH to around pH10.
And more metals removed when we bring the salt solution back to neutral around pH 7...

 

[Goldman94]

I do not understand why your working with two batches?
It is hard for me to follow all of what is going on, I thought you were working with one mess, not two different batches.

Well as long as you understand what your doing.

After collecting all of your washes and solutions (even if they test negative for gold) you will not lose your gold if you follow the instructions to treat your waste for disposal properly. found in the safety section...

Any gold will cement out with copper. You will recover it in this step.
Copper and many of the other toxic base metals are cemented out with an iron.
Many more of the toxic metals are removed by raising the pH to around pH10.
And more metals removed when we bring the salt solution back to neutral around pH 7...

So when I was processing everything the other day, before this all happened. I split the AR solutions into 2 batches. One ended up being a golden yellow color and the other ended up being a dark brown color. I did the exact same stuff with both so I was confused as to why they were different colors

 

[butcher]

you may have done the exact same thing, but apparently the chemical reactions formed slightly different.

They could hold different salts of metals, possibly some in different oxidation states, could have previously held different gases, and have made different reactions, possibly the salts may be in different pH ranges...
At this point, colors do not mean much.

 

[Goldman94]

you may have done the exact same thing, but apparently the chemical reactions formed slightly different.

They could hold different salts of metals, possibly some in different oxidation states, could have previously held different gases, and have made different reactions, possibly the salts may be in different pH ranges...
At this point, colors do not mean much.

It's weird though, since it seems like a good majority of the gold is in the 'good' beaker and it doesnt seem like much is in the other one. There's a little in there but definitely not as much as the yellow one. There's a nice layer of solid gold and, what I hope to be, gold powder at the bottom of this one.

Tomrrow I will try to process it with AR and proceed from that step, adding in nitric little by little this time.

I believe I have gotten most of the salts out of the solution by adding the water and evaporating them, but if theres still some traces left, how will that affect the AR solution?

 

[butcher]

I would keep everything in one batch and process it together if you have two batch's you have two sources to lose a little bit gold in each batch, the more small batches, with the small losses in each, which adds up over time.

It is better to work with larger batches and keep all of the chemical reactions in one pot as much as possible keeping your eggs in one nest as much as possible and not spread all over the lab...

I put my gold in a corning dish on a hot plate and rarely take it out during recovery and refining, It will see some glassware and filters before being melted, but the gold is pretty much done in the same pot throughout the processes, in one batch keeping the gold in one nest as much as possible.

Traces, or a small amount that will not dissolve after you finish with the recommended process of washing your gold to get it pure and shiny, I would not worry about it, you will clean up the gold more after the second refining.

You may also consider not using aqua regia the next go-around, the gold will be fine enough for HCl and bleach to easily put it into solution after you do a proper washing procedure.